CN114890408B - Preparation method of carbon nano tube with controllable size distribution and preparation method of carbon nano tube reinforced aluminum matrix composite material - Google Patents
Preparation method of carbon nano tube with controllable size distribution and preparation method of carbon nano tube reinforced aluminum matrix composite material Download PDFInfo
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Abstract
The application relates to a preparation method of a carbon nano tube with controllable size distribution, which comprises the steps of adjusting the size of nano metal particles and the volume ratio of the nano metal particles to an original carbon nano tube, enabling the distribution of the nano metal particles to meet the size distribution rule of the required carbon nano tube after the nano metal particles are plated on the surface of the acidized carbon nano tube, and then enabling the carbon nano tube plated with the nano metal particles to be broken down by adjusting the power and time of microwave discharge, thus obtaining the carbon nano tube with the required size distribution with good dispersibility. The application also relates to a method for preparing the aluminum-based composite material by using the carbon nano tube obtained by the method.
Description
Technical Field
The application relates to the technical field of carbon nanotubes, in particular to a preparation method of a carbon nanotube with controllable size distribution and a preparation method of a carbon nanotube reinforced aluminum matrix composite material.
Background
The carbon nano tube is formed by sp 2 The one-dimensional carbon material formed by hybridized C=C covalent bonds has extremely high modulus, strength and toughness, the Young modulus of a single carbon nano tube can reach 1.8TPa, the tensile strength can reach 6.0GPa, and 15% of tensile strain can be generated before fracture. The carbon nanotube preparation method mainly comprises arc discharge method, laser ablation method, chemical vapor deposition method, solid phase pyrolysis method, glow discharge method, gas combustion method, polymerization synthesis method, etc. Although the method can prepare the carbon nano tube, the prepared carbon nano tube has stronger van der Waals force and larger length-diameter ratio, is easy to wind together or agglomerate into a bundle, cannot control the size distribution of the carbon nano tube, and limits the application of the carbon nano tube.
Disclosure of Invention
Based on the above, it is necessary to provide a preparation method of carbon nanotubes with controllable size distribution, which has good dispersibility, aiming at the problems that the carbon nanotubes obtained by the conventional preparation method are easy to agglomerate and the size distribution of the carbon nanotubes cannot be controlled.
A preparation method of a carbon nano tube with controllable size distribution comprises the following steps:
providing pristine carbon nanotubes and nano-metal particles;
according to the size distribution rule of the required carbon nano tube, the size of the nano metal particles and the volume ratio of the nano metal particles to the original carbon nano tube are adjusted;
acidizing the original carbon nano tube, and plating nano metal particles on the surface of the acidized carbon nano tube;
and carrying out microwave plasma discharge treatment on the carbon nano tube plated with the nano metal particles, and adjusting the power and time of microwave discharge so as to break down the carbon nano tube plated with the nano metal particles and obtain the carbon nano tube with the required size distribution.
In one embodiment, the length of the pristine carbon nanotubes is 0.5 μm to 500 μm.
In one embodiment, the desired carbon nanotubes have a size distribution pattern of: carbon nanotubes with average length of 100 nm-1000 nm and carbon nanotubes with average length of 1 μm-100 μm are distributed according to volume ratio of 1:1-10:1.
In one embodiment, the nano-metal particles are tunable in size in the range of 0.1nm to 300nm.
In one embodiment, the volume content of the nano metal particles relative to the original carbon nanotubes is adjustable within a range of 0.1% -80%.
In one embodiment, the microwave discharge has a power of 0.01mW/cm 3 ～300mW/cm 3 Adjustable in range; the time of microwave discharge is adjustable within the range of 0.1-30 seconds.
In one embodiment, the acid solution used in the acidification treatment is nitric acid, sulfuric acid or a mixture of sulfuric acid and nitric acid, and the acidification treatment time is 2-10 hours.
In one embodiment, the nano-metal particles are gold, silver, copper, iron, tungsten, tin, aluminum, or titanium.
In one embodiment, the plating is performed by electroless plating, spray pyrolysis, electroplating, chemical vapor deposition, physical vapor deposition, evaporation, or ion sputtering.
According to the preparation method of the carbon nano tube with controllable size distribution, the size of the nano metal particles and the volume content of the nano metal particles relative to the original carbon nano tube are adjusted, so that the distribution of the nano metal particles after the nano metal particles are plated on the surface of the acidized carbon nano tube meets the size distribution rule of the required carbon nano tube, and then the carbon nano tube plated with the nano metal particles is broken down by adjusting the power and time of microwave discharge, so that the carbon nano tube with the required size distribution with good dispersibility is obtained.
The method can realize the matching and combination of long and short carbon nanotubes in any proportion, and as metal particles are plated at the breakdown part, the compatibility of the carbon nanotubes and the contact phase boundary of the metal can be further improved, the wettability between the carbon nanotubes and the metal matrix is enhanced, the agglomeration of the carbon nanotubes is reduced, and the preparation of the carbon nanotube hybrid enhanced metal matrix composite material with different lengths is realized.
Therefore, the application also provides a preparation method of the carbon nano tube reinforced aluminum matrix composite, which comprises the following specific scheme:
a preparation method of a carbon nano tube reinforced aluminum matrix composite material comprises the following steps:
preparing the carbon nano tube with the required size distribution by adopting the preparation method of any one of the above steps;
and uniformly mixing the carbon nano tube with the required size distribution with the aluminum-based powder, and sintering to obtain the carbon nano tube reinforced aluminum-based composite material.
In one embodiment, the carbon nanotubes of the desired size distribution are distributed from carbon nanotubes having an average length of 100nm to 1000nm and carbon nanotubes having an average length of 1 μm to 100 μm at a volume ratio of 1:1 to 10:1.
In one embodiment, the volume content of the carbon nanotubes in the carbon nanotube reinforced aluminum matrix composite is 0.1% -30%.
In one embodiment, the sintering is performed by a method selected from at least one of hot pressing, plasma activated sintering, isostatic pressing, vacuum sintering, and atmospheric sintering.
In one embodiment, the step of sintering is further followed by a step of post-processing, the post-processing being selected from at least one of hot pressing, hot extrusion, and forging.
The preparation method of the carbon nano tube reinforced aluminum matrix composite material can realize the carbon nano tube hybrid reinforced aluminum matrix composite materials with different sizes according to the needs, is simple and easy to control, and can be applied to actual industrial production.
Drawings
FIG. 1 is a TEM image of a carbon nanotube prior to electroless copper plating;
FIG. 2 is a TEM image of a carbon nanotube after electroless copper plating;
FIG. 3 is a stress-strain diagram of an aluminum-based composite material with a carbon nanotube volume content of 2.5% and a matrix;
fig. 4 is an SEM image of a surface-plated W carbon nanotube prepared by spray pyrolysis.
Detailed Description
The present application will be described more fully hereinafter in order to facilitate an understanding of the present application, and preferred embodiments of the present application are set forth. This application may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The preparation method of the carbon nano tube with controllable size distribution in one embodiment comprises the following steps S110 to S140:
s110, providing the original carbon nano-tubes and nano-metal particles.
Wherein the original carbon nano tube is a single carbon nano tube, and the length is 0.5-500 mu m.
Further, the length of the original carbon nanotube is 20 μm to 30 μm and 80 μm to 100 μm.
It is understood that the length of the original carbon nanotubes can be adjusted according to the size distribution rule of the desired carbon nanotubes, and is not limited to the above-mentioned limitation.
The nano metal particles are gold (Au), silver (Ag), copper (Cu), iron (Fe), tungsten (W), tin (Sn), aluminum (Al) or titanium (Ti).
The size of the nano metal particles is 0.1 nm-300 nm.
Further, the size of the nano metal particles is 5nm to 10nm.
It is understood that the size of the nano-metal particles can be adjusted according to the size distribution rule of the desired carbon nanotubes, and is not limited to the above-limited range.
S120, according to the size distribution rule of the required carbon nano tube, the size of the nano metal particles and the volume content of the nano metal particles relative to the original carbon nano tube are adjusted.
The size of the nano metal particles and the volume content of the nano metal particles relative to the original carbon nano tube are key factors for obtaining the carbon nano tube with the required size distribution rule, and the carbon nano tube with the average length of 100 nm-1000 nm and the average length of 1 mu m-100 mu m can be distributed according to the ratio of 1:1-10:1 by controlling the size of the nano metal particles to be in the range of 0.1 nm-300 nm and the volume content of the nano metal particles relative to the original carbon nano tube to be in the range of 0.1% -80%.
S130, acidizing the original carbon nano tube, and plating nano metal particles on the surface of the acidized carbon nano tube.
Wherein the acid liquor used for the acidification treatment is sulfuric acid, nitric acid or a mixture of sulfuric acid and nitric acid. The acidification treatment time is 2-10 hours.
Further, sulfuric acid is an aqueous sulfuric acid solution with a mass content of not less than 70%, and nitric acid is an aqueous nitric acid solution with a mass content of not less than 68%. The volume ratio of sulfuric acid to nitric acid in the mixture is 1:1-1:3.
The plating adopts the methods of chemical plating, spray pyrolysis, electroplating, chemical vapor deposition, physical vapor deposition, evaporation plating or ion sputtering, etc.
It should be noted that, the nano metal particles may be plated on the surface of the carbon nanotube after the acidification treatment by any method known in the art, and is not limited to the above-listed methods.
And S140, performing microwave plasma discharge treatment on the carbon nano tube plated with the nano metal particles, and adjusting the power and time of microwave discharge so as to break down the carbon nano tube plated with the nano metal particles and obtain the carbon nano tube with the required size distribution.
Wherein the microwave discharge power is 0.01mW/cm 3 ～300mW/cm 3 Within the range ofIs adjustable. The time of microwave discharge is adjustable within the range of 0.1-30 seconds.
The power and the time of microwave discharge are controlled, so that the carbon nano tube plated with nano metal particles is broken down and the ablation and the damage of the carbon nano tube structure are not caused.
According to the preparation method of the carbon nano tube with controllable size distribution, after the size of the nano metal particles and the volume ratio of the nano metal particles to the original carbon nano tube are adjusted according to the size distribution rule of the carbon nano tube, the distribution of the nano metal particles after the nano metal particles are plated on the surface of the acidized carbon nano tube meets the size distribution rule of the carbon nano tube, and then the carbon nano tube plated with the nano metal particles is broken down by adjusting the power and time of microwave discharge, so that the carbon nano tube with the required size distribution with good dispersibility can be obtained.
The method can realize the matching and combination of long and short carbon nanotubes in any proportion, and as metal particles are plated at the breakdown part, the compatibility of the carbon nanotubes and the contact phase boundary of the metal can be further improved, the wettability between the carbon nanotubes and the metal matrix is enhanced, the agglomeration of the carbon nanotubes is reduced, and the preparation of the carbon nanotube hybrid enhanced metal matrix composite material with different lengths is realized.
The preparation method of the carbon nano tube reinforced aluminum matrix composite in one embodiment comprises the following steps S210 to S220:
s210, providing carbon nanotubes with the required size distribution.
It is understood that the carbon nanotubes with the desired size distribution can be prepared according to the steps S110 to S140, and will not be described herein.
And S220, uniformly mixing the carbon nano tube with the required size distribution with the aluminum-based powder, and sintering to obtain the carbon nano tube reinforced aluminum-based composite material.
Wherein the aluminum-based powder is pure aluminum powder or aluminum alloy powder. The volume content of the carbon nano tube in the obtained carbon nano tube reinforced aluminum matrix composite is 0.1-30%.
The sintering temperature is 550-700 ℃.
It should be noted that, in the step S220, sintering is a densification process, and any sintering method known in the prior art may be selected by those skilled in the art according to need, for example, one or more of hot press sintering, plasma activated sintering, isostatic pressing sintering, vacuum sintering and atmosphere sintering may be selected to densify the mixed powder and increase the strength.
In addition, the man skilled in the art can also carry out post-processing treatments such as hot pressing, hot extrusion, rolling, forging, etc. after the sintering step, as required, to further improve the mechanical properties of the material.
The preparation method of the carbon nano tube reinforced aluminum matrix composite material can realize the carbon nano tube hybrid reinforced aluminum matrix composite materials with different sizes according to the needs, is simple and easy to control, and can be applied to actual industrial production.
The carbon nano tube reinforced aluminum matrix composite material prepared by the method has the advantages that the carbon nano tube reinforced phase is uniformly dispersed, the wettability with a matrix is good, and compared with the carbon nano tube reinforced aluminum matrix composite material prepared by the traditional method, the comprehensive performance is effectively improved.
The following are specific examples.
Example 1
(1) Preparation of carbon nanotubes of desired size distribution
The size distribution rule of the required carbon nano tube is as follows: carbon nanotubes having an average size of 100nm and carbon nanotubes having an average size of 30 μm were distributed at a volume ratio of 1:1.
The length of the original carbon nano tube is 80-100 mu m, the size of the nano Cu particles is 5-10 nm, and the volume content of the nano Cu particles relative to the original carbon nano tube is 10%.
The preparation method comprises the following steps: acidifying the original carbon nano tube with concentrated nitric acid for 2 hours, and placing the acidified carbon nano tube into 0.1mol/L SnCl by adopting a chemical plating method 2 Stirring for 2h, standing, separating, washing to neutrality, and adding 0.01g/L PdCl 2 Stirring for 2h, standing, separating, and washing to neutrality to obtain the carbon nanotube dispersion liquid. The main salt CuSO 4 ·5H 2 O is dissolved inAdding complexing agent KNaC into proper amount of deionized water 4 H 4 O 6 ·4H 2 And O, adding NaOH solution to adjust the pH value to 9-10, finally adding polyethylene glycol (M=1000), dripping the polyethylene glycol and formaldehyde aqueous solution (HCHO, 37%) into the carbon nanotube dispersion liquid at a constant speed, washing and drying to obtain the carbon nanotube plated with the nano Cu particles.
Performing microwave plasma discharge treatment on the obtained carbon nano tube plated with nano Cu particles, and adjusting the power of microwave discharge to 0.01mW/cm 3 And (5) continuously discharging for 30 seconds to obtain the carbon nano tube with the required size distribution.
Referring to fig. 1 to 2, TEM images of carbon nanotubes before and after electroless copper plating are shown. As can be seen from fig. 1 to 2, cu particles have a size of about 10nm and are covered and interpenetrated in the middle of the carbon nanotubes.
(2) Preparation of carbon nano tube reinforced aluminium base composite material
And (3) ball-milling and mixing the carbon nano tube with the required size distribution obtained in the step (1) and pure aluminum powder, and performing hot extrusion after plasma activated sintering at 550 ℃ to obtain the carbon nano tube reinforced aluminum matrix composite material. The volume content of the carbon nano tube in the composite material is 2.5 percent.
FIG. 3 is a stress-strain diagram of an aluminum-based composite material with a carbon nanotube volume content of 2.5% and a matrix. As can be seen from fig. 3, the addition of carbon nanotubes can significantly improve the strength of the matrix.
Example 2
(1) Preparation of carbon nanotubes of desired size distribution
The size distribution rule of the required carbon nano tube is as follows: carbon nanotubes having an average length of 500nm and carbon nanotubes having an average length of 5 μm were distributed at a volume ratio of 1:1.
The length of the original carbon nano tube is 20-30 mu m, the size of the nano W particles is 200nm, and the volume content of the nano W particles relative to the original carbon nano tube is 50%.
The preparation method comprises the following steps: acidifying the original carbon nano tube for 10 hours by adopting concentrated sulfuric acid, adding the acidified carbon nano tube into 3g/L ammonium meta-tungstate aqueous solution by adopting a spray pyrolysis method, stirring for 30min to prepare a precursor liquid, pouring the precursor liquid into an ultrasonic atomizer to be atomized into tiny liquid drops, and carrying out spray pyrolysis furnace on the tiny liquid drops along with air flow at 750 ℃ and then carrying out hydrogen reduction to obtain the carbon nano tube plated with nano W particles.
Performing microwave plasma discharge treatment on the obtained carbon nano tube plated with the nano W particles, and adjusting the power of microwave discharge to be 100mW/cm 3 Intermittent discharge is carried out for 30 seconds, and the interval time is 5 seconds, so that the carbon nano tube with the required size distribution is obtained.
Fig. 4 is an SEM image of surface-plated W particles prepared by spray pyrolysis. As can be seen from FIG. 4, the W particles are between 20nm and 30nm in size.
(2) Preparation of carbon nano tube reinforced aluminium base composite material
And (3) ball-milling and mixing the carbon nano tube with the required size distribution obtained in the step (1) and 2024 aluminum alloy powder, hot-pressing and sintering at 700 ℃, and rolling to obtain the carbon nano tube reinforced aluminum matrix composite. The volume content of the carbon nano tube in the carbon nano tube reinforced aluminum matrix composite is 1.0 percent
Through detection, the tensile strength of the carbon nano tube reinforced aluminum matrix composite material prepared in the step (2) is 400MPa, and the tensile strength is improved by nearly 1 time compared with a matrix.
Comparative example 1
Comparative example 1 was substantially the same as example 2 except that the carbon nanotubes having the desired size distribution in step (2) were commercially available carbon nanotubes having a size of 30 μm to 50. Mu.m.
The tensile strength of the carbon nano tube reinforced aluminum matrix composite prepared in the comparative example 2 is only 280MPa.
Example 3
(1) Preparation of carbon nanotubes of desired size distribution
The size distribution rule of the required carbon nano tube is as follows: carbon nanotubes having an average length of 5nm to 60 nm.
The length of the original carbon nano tube is 20-30 mu m, the size of the nano Fe particles is 150nm, and the volume content of the nano Fe particles relative to the original carbon nano tube is 30%.
The preparation method comprises the following steps: acidifying the original carbon nano tube for 8 hours by adopting a mixed solution of nitric acid and sulfuric acid, placing the acidified carbon nano tube at the tail end of a tube furnace by adopting a chemical vapor deposition method, introducing carbon monoxide reducing gas, placing an iron powder raw material (325 meshes) at the central position of the tube furnace, taking out after a certain time, heating to 280 ℃ in a vacuum environment, and preserving heat for 40 minutes to obtain the carbon nano tube plated with nano Fe particles.
Performing microwave plasma discharge treatment on the obtained carbon nano tube plated with nano Fe particles, and adjusting the power of microwave discharge to 200mW/cm 3 And the discharge is continued for 20 seconds, so that the carbon nano tube with good dispersibility and required size distribution is obtained.
(2) Preparation of carbon nano tube reinforced aluminium base composite material
And (3) ball-milling and mixing the carbon nano tube with the required size distribution obtained in the step (1) and pure aluminum powder, and hot-pressing and sintering at 600 ℃ to obtain the carbon nano tube reinforced aluminum matrix composite. The volume content of the carbon nano tube in the carbon nano tube reinforced aluminum matrix composite is 5%.
Comparative example 2
Comparative example 2 was substantially the same as example 3 except that the carbon nanotubes having the desired size distribution in the step (2) were commercially available carbon nanotubes having a size of 30 μm to 50. Mu.m.
According to detection, compared with the carbon nano tube reinforced aluminum matrix composite material prepared in comparative example 2, the tensile strength of the carbon nano tube reinforced aluminum matrix composite material prepared in example 3 is improved by 30%.
Example 4
(1) Preparation of carbon nanotubes of desired size distribution
The size distribution rule of the required carbon nano tube is as follows: carbon nanotubes having an average size of 100nm and carbon nanotubes having an average size of 50 μm were distributed at a volume ratio of 10:1.
The length of the original carbon nano tube is 50 mu m, the size of the nano Sn particles is 150nm, and the volume content of the nano Sn particles relative to the original carbon nano tube is 80%.
The preparation method comprises the following steps: acidifying the original carbon nano tube for 4 hours by adopting concentrated nitric acid, placing the acidified carbon nano tube on a substrate table of a sputtering cavity by adopting a magnetron sputtering method, and vacuumizing the cavity until the original carbon nano tube is vacuumized5×10 -4 Argon is introduced at a constant flow rate and below Pa. Setting the rotation speed of a sample table to be 10r/min, adopting pure tin as a target material, wherein the purity is more than 99.9%, the distance between the target electrodes is 8cm, and the power and the working air pressure of radio frequency sputtering are respectively 50W and 0.6Pa, so as to obtain the carbon nano tube plated with nano Sn particles.
Performing microwave plasma discharge treatment on the obtained carbon nano tube plated with nano Sn particles, and adjusting the power of microwave discharge to 300mW/cm 3 And (3) continuously discharging for 30 seconds to obtain the carbon nano tube with good dispersibility and required size distribution.
(2) Preparation of carbon nano tube reinforced aluminium base composite material
And (3) ball-milling and mixing the carbon nano tube with the required size distribution obtained in the step (1) and pure aluminum powder, and performing vacuum sintering at 700 ℃ and hot extrusion to obtain the carbon nano tube reinforced aluminum matrix composite. The volume content of the carbon nano tube in the composite material is 30%.
The foregoing examples illustrate only a few embodiments of the application and are described in detail herein without thereby limiting the scope of the application. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the application, which are all within the scope of the application. Accordingly, the scope of protection of the present application is to be determined by the appended claims.
Claims (7)
1. The preparation method of the carbon nano tube with controllable size distribution is characterized by comprising the following steps of:
providing pristine carbon nanotubes and nano-metal particles;
according to the size distribution rule of the required carbon nano tube, the size of the nano metal particles and the volume content of the nano metal particles relative to the original carbon nano tube are adjusted;
acidizing the original carbon nano tube, and plating nano metal particles on the surface of the acidized carbon nano tube;
performing microwave plasma discharge treatment on the carbon nanotubes plated with the nano metal particles, and adjusting the power and time of microwave discharge so as to break down the carbon nanotubes plated with the nano metal particles to obtain the carbon nanotubes with the required size distribution;
the size distribution rule of the required carbon nano tube is as follows: carbon nanotubes with average length of 100 nm-1000 nm and carbon nanotubes with average length of 1 μm-100 μm are distributed according to the volume ratio of 1:1-10:1;
the size of the nano metal particles is adjustable within the range of 0.1 nm-300 nm; the volume content of the nano metal particles relative to the original carbon nano tube is adjustable within the range of 0.1-80%;
the power of the microwave discharge is 0.01mW/cm 3 ～300mW/cm 3 Adjustable in range; the time of microwave discharge is adjustable within the range of 0.1-30 seconds.
2. The method for producing carbon nanotubes with controllable size distribution according to claim 1, wherein the length of the raw carbon nanotubes is 0.5 μm to 500 μm.
3. The method for preparing carbon nanotubes with controllable size distribution according to claim 1 or 2, wherein the acid solution used in the acidification treatment is nitric acid, sulfuric acid or a mixture of sulfuric acid and nitric acid, and the acidification treatment time is 2-10 hours.
4. The method for preparing carbon nanotubes with controllable size distribution according to claim 1 or 2, wherein the nano metal particles are gold, silver, copper, iron, tungsten, tin, aluminum or titanium.
5. The method for preparing the carbon nanotubes with controllable size distribution according to claim 1 or 2, wherein the plating is performed by electroless plating, spray pyrolysis, electroplating, chemical vapor deposition, physical vapor deposition, evaporation or ion sputtering.
6. The preparation method of the carbon nano tube reinforced aluminum matrix composite material is characterized by comprising the following steps of:
preparing carbon nanotubes with the required size distribution by adopting the preparation method of the carbon nanotubes with controllable size distribution as claimed in any one of claims 1 to 5;
and uniformly mixing the carbon nano tube with the required size distribution with the aluminum-based powder, and sintering to obtain the carbon nano tube reinforced aluminum-based composite material.
7. The method for preparing a carbon nanotube-reinforced aluminum matrix composite according to claim 6, wherein the carbon nanotube-reinforced aluminum matrix composite has a volume content of 0.1% to 30%; the sintering temperature is 550-700 ℃.
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